HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → HCID 59532407, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | 2-Chloro-5-pyridinesulfonyl chloride | HCID 2792792 | — |
| Reactant | tert-butyl (2S)-4-[(4-amino-2-methylphenyl)methyl]-2-methylpiperazine-1-carboxylate | HCID 59262126 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Water methylene chloride | HCID 21908982 | — |
| Product | HCID 59532407 | HCID 59532407 | 106.8% |
Reaction Steps
D7 (100 mg, 0.31 mmol) in dry DCM (1.05 mL) and pyridine (0.30 mL, 3.8 mmol) was stirred to 0° C. under argon and 6-chloro-3-pyridinesulfonyl chloride (60 mg, 0.28 mmol) in dry DCM (1.05 mL) added dropwise. The reaction mixture was stirred under argon and allowed to warm to room temperature. After 17 h, the reaction mixture was diluted with water/DCM. The aqueous layer was extracted with DCM, the organic layer dried (Na2SO4) and solvent removed under vacuum. The product was purified by column chromatography (Biotage Horizon 40+S) eluting with petroleum ether/Et2O to afford the title compound as a colourless oil (148 mg). MS (ES+): MH+ 495.1/497.1.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07964597B2 |
| Source dataset | uspto-grants-2011_06 |
| ORD ID | ord-8ef75575d93c4cf39b05c8bcc1a5c2b8 |
| Source note | uspto-grants-2011_06 |